CN206666136U - A kind of device for preparing graphene - Google Patents

A kind of device for preparing graphene Download PDF

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Publication number
CN206666136U
CN206666136U CN201720332225.6U CN201720332225U CN206666136U CN 206666136 U CN206666136 U CN 206666136U CN 201720332225 U CN201720332225 U CN 201720332225U CN 206666136 U CN206666136 U CN 206666136U
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Prior art keywords
reaction vessel
graphene
preparing graphene
fixed plate
expanded graphite
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CN201720332225.6U
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Chinese (zh)
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张金玉
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Harbin Ferry New Material Co Ltd
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Harbin Ferry New Material Co Ltd
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Abstract

A kind of device for preparing graphene, described device includes the first reaction vessel and the second reaction vessel connected by water pump, first reaction vessel and the second reaction container bottom are full of weak acid electrolyte in the reaction vessel of metallic plate first, the outer surface of expanded graphite cake is welded with conductive metal mesh, platinum filament fixed plate is inlaid in the top of the second reaction vessel, and the inner surface of platinum filament fixed plate is welded with some platinum filaments vertically.The utility model mainly make use of the principle of electrolysis, one end using expanded graphite as conductive electrode, it is electrolysed in access circuit, so that expanded graphite is successively peeled off in the electrolytic solution, electrolyte is subjected to re-electrolysis by platinum filament again, peeled off after cleaning with ultrasonic wave, then dry and just obtained required graphene.And in obtained graphene, the proportion that single-layer graphene accounts for is very big.

Description

A kind of device for preparing graphene
Technical field
The utility model belongs to technical field of graphene preparation, and in particular to a kind of to prepare graphene using expanded graphite Device.
Background technology
Native graphite alkene is the two dimensional crystal for being stripped out from graphite material, being made up of carbon atom.Graphene is both Most thin material, and most tough material, 200 times more taller than best steel of fracture strength.It has well again simultaneously Elasticity, stretch range can reach the 20% of own dimensions.It is that current nature is most thin, intensity highest material, graphene mesh Preceding most potential application is the substitute as silicon, manufactures ultra micro transistor npn npn, for producing the supercomputer in future.With Graphene substitutes silicon, and the speed of service of computer processor will be fast hundreds times.In addition, graphene is almost fully transparent, Only absorb 2.3% light.On the other hand, it is very fine and close, even minimum gas atom (helium atom) can not also penetrate.This A little features cause it to be highly suitable as the raw material of transparent electron product, such as transparent touch display screen, luminescent screen and solar energy Cell panel.A kind of novel nano-material most strong as the most thin, maximum intensity, electrical and thermal conductivity performance that have now been found that, graphene It is referred to as " dark fund ", is " king of new material ", scientist even foretells that graphene " will thoroughly change 21 century ".
In the prior art, the synthetic method of graphene mainly has two kinds:Mechanical means and chemical method.Mechanical means includes Mechanical phonograph recorder separation, epitaxy method and the method for heating SiC, chemical method is chemical reduction method and chemical dissociation method.
Most common is micromechanics partition method, directly cuts down graphene platelet from larger crystal.2004 Novoselovt etc. has prepared single-layer graphene in this way, and can be stabilized under external environment.It is prepared by typical case Method be with another material it is expanded or introduce defect pyrolytic graphite rubbed, the surface of body phase graphite can produce wadding The crystal of sheet, the graphene containing individual layer in the crystal of these flocculus shapes.But shortcoming is that this method is to utilize the graphite table that rubs The thin slice that face obtains filters out the graphene platelet of individual layer, and its size is difficult to control, and reliably can not supply enough factory length Graphite flake sample.
Epitaxy method is to go out graphene using growth substrate atomic structure " kind ", allows carbon atom to be oozed at 1150 DEG C first Enter ruthenium, then cool down, after being cooled to 850 DEG C, a large amount of carbon atoms absorbed before will float to ruthenium surface, the individual layer of lens shape Carbon atom " isolated island " be covered with whole stromal surface, it is final they can grow up to a complete layer graphene.First layer covers After 80%, the second layer starts to grow.The graphene of bottom can produce strong reciprocation with ruthenium, and after the second layer just almost with Ruthenium is kept completely separate, only remaining light current coupling, and obtained single-layer graphene thin slice performance is satisfactory.But produce in this way Graphene platelet it is often in uneven thickness, and the bonding between graphene and matrix can influence the characteristic of carbon-coating.
Chemical reduction method is to mix graphite oxide and water with 1mg/mL ratio, with supersonic oscillations to the clear nothing of solution Particulate material, appropriate hydrazine is added in 100 DEG C of backflow 24h, generation black particle shape precipitation, filtering, drying graphene.Change It is the method that graphite oxide is prepared to graphene by the method for thermal reduction to learn dissociation method, the oxygen-containing functional group of graphite oxide interlayer React at a certain temperature.
Wherein, electrolysis be it is the most frequently used prepare the method for graphene, but have that graphene yield is too low, and purity is not high The problem of.
Utility model content
The purpose of this utility model is to solve in existing graphene preparation technology, and graphene yield is too low, and purity is not The problem of high, and then a kind of device for preparing graphene is provided.
The technical solution of the utility model is:
A kind of device for preparing graphene, described device include the first reaction vessel 1 and second connected by water pump 11 Reaction vessel 8, the first reaction vessel 1 and the bottom of the second reaction vessel 8 are embedded with metallic plate 4, are full of in the first reaction vessel 1 weak Acid electrolyte 5, expanded graphite cake 2 are placed in the top of the first reaction vessel 1, and the outer surface of expanded graphite cake 2 is welded with conducting metal Net 3, platinum filament fixed plate 9 are placed in the top of the second reaction vessel 8, and the inner surface of platinum filament fixed plate 9 is welded with some platinum filaments 10 vertically, The positive pole of power supply 6 is connected with conductive metal mesh 3 and platinum filament fixed plate 9 respectively by wire, and the negative pole of power supply 6 passes through wire and two Block metallic plate 4 connects.
Further, the expanded graphite cake 2 is placed in the top of the first reaction vessel 1 with suspension bracket.
Further, glue sticking is used between the reaction vessel 1 of conductive metal sheet 4 and first.
Further, the platinum filament fixed plate 9 is placed in the top of the second reaction vessel 8 with suspension bracket.
Further, weak acid electrolyte 5 is the weak acid such as dilute oxalic acid or dilute sulfuric acid.
Further, the material of the first reaction vessel 1 and the second reaction vessel 8 is non-conductive.
Further, the material of conductive metal mesh 3 and conductive metal sheet 4 is copper, iron or aluminium.
Further, the voltage of power supply 6 is 5 to 30 volts.
The utility model has the advantages that:The utility model mainly make use of the principle of electrolysis, by expanded graphite As one end of conductive electrode, accessing in circuit and be electrolysed so that expanded graphite is successively peeled off in the electrolytic solution, then by electricity Solve liquid and re-electrolysis is carried out by platinum filament, then filter cleaning, drying and just obtained required graphene.And obtained graphite In alkene, the proportion that single-layer graphene accounts for is very big.Such a method is simple and easy, requires low to device, it is not necessary to complicated manipulator Section can be completed, and be worthy to be popularized.
Brief description of the drawings
Fig. 1 is the schematic diagram for the device that the utility model electrolysis prepares graphene.
Embodiment
Illustrate present embodiment with reference to Fig. 1, present embodiment includes a kind of device for preparing graphene, and described device includes The first reaction vessel 1 and the second reaction vessel 8 connected by water pump 11, the first reaction vessel 1 and the bottom of the second reaction vessel 8 Embedded with metallic plate 4, weak acid electrolyte 5 is full of in the first reaction vessel 1, expanded graphite cake 2 is inlaid in the top of reaction vessel 1 Portion, the outer surface of expanded graphite cake 2 are welded with conductive metal mesh 3, and platinum filament fixed plate 9 is inlaid in the top of the second reaction vessel 8, platinum The inner surface of silk fixed plate 9 is welded with some platinum filaments 10 vertically, the positive pole of power supply 6 by wire respectively with conductive metal mesh 3 and platinum Silk fixed plate 9 is connected, and the negative pole of power supply 6 is connected by wire with two pieces of metallic plates 4.
Preferably, connected between expanded graphite cake 2 and reaction vessel 1 with suspension bracket.The conductive metal sheet 4 and reaction vessel Glue sticking is used between 1.Connected between platinum filament fixed plate 2 and reaction vessel 1 with suspension bracket.
Weak acid electrolyte 5 is preferably dilute oxalic acid or dilute sulfuric acid.The material of reaction vessel 1 is non-conductive, can preferred glass Container.The preferred copper of the material of conductive metal mesh 3 and conductive metal sheet 4, the iron either common metal such as aluminium or graphite cake.Power supply 6 Voltage be preferably 5 to 30 volts.
The preparation method of expanded graphite cake 2 is as follows:
Natural flake graphite is taken, in the mixed acid solution of sulfuric acid and nitric acid is added under being stirred continuously, adds Gao Meng Sour potassium, certain temperature is controlled, then adds ferric trichloride, stirred, after reacting certain time, centrifuged, use dilute alkaline soln Embathe, be washed to acidity, high-temperature expansion is dried again after dehydration can obtain expanded graphite worm.Need that stone will be expanded further according to device Ink is tightly compacted to be can be used into different shape.
The utility model also includes a kind of method that graphene is prepared using said apparatus, comprises the following steps:By conduction Metallic plate 4 is inlaid in the bottom of reaction vessel 1, then weak acid electrolyte 5 is full of into reaction vessel 1, then that expanded graphite cake 2 is embedding Mounted in the top of reaction vessel 1, power supply 6 is connected by wire with conductive metal mesh 3 and conductive metal sheet 4 respectively, turns on the power 6 Switch is electrolysed to expanded graphite cake 2, and fully after electrolysis, weak acid electrolyte 5 is evacuated into the second reaction vessel 8 by water pump 11 It is interior;
The positive pole of power supply 6 is connected by wire with platinum filament fixed plate 9, and the negative pole of power supply 6 is connected by wire and metallic plate 4 Connect, turn on the power 6 switches and the graphene in weak acid electrolyte 5 is electrolysed again, fully after electrolysis, by graphene and electrolysis The mixture of liquid cleans after taking out, then is filtered after ultrasonication stripping, that is, obtains required graphene.
The principle of present embodiment:Power supply 6 leads to 5 to 30 volt voltages, and conductive metal mesh 3 can be electrolysed expanded graphite cake after being powered 2, graphene is peeled off into, is extracted out using water pump from from reaction vessel 1 in the reaction vessel of weak acid electrolyte 5 to the second 8, platinum The expanded graphite that the energization of silk 10 can make not to be electrolysed fully in electrolyte is electrolysed again, graphene is peeled off into, then from second The mixture of weak acid electrolyte 5 and graphene is poured out in reaction vessel 8, mixture is cleaned using filter, is utilized Ultrasonic wave carries out ultrasound to the graphene filtered out, then peels off filtering, and graphene is dried using dryer, completes graphene Electrolytic preparation.The method is simple and easy and single-layer graphene accounting is very high.
The above is only preferred embodiment of the present utility model, is not intended to limit embodiment of the present utility model, Those of ordinary skill in the art can very easily carry out corresponding accommodation according to central scope of the present utility model and spirit Or modification, therefore the scope of protection of the utility model should be defined by the protection domain required by claims.

Claims (7)

1. a kind of device for preparing graphene, it is characterised in that described device includes the first reaction connected by water pump (11) Container (1) and the second reaction vessel (8), the first reaction vessel (1) and the second reaction vessel (8) bottom are embedded with metallic plate (4), Weak acid electrolyte (5) is full of in first reaction vessel (1), expanded graphite cake (2) is placed in the top of the first reaction vessel (1), swollen The outer surface of swollen graphite cake (2) is welded with conductive metal mesh (3), and platinum filament fixed plate (9) is placed in the top of the second reaction vessel (8), The inner surface of platinum filament fixed plate (9) is welded with some platinum filaments (10) vertically, the positive pole of power supply (6) by wire respectively with conducting metal Net (3) and platinum filament fixed plate (9) connection, the negative pole of power supply (6) are connected by wire with two pieces of metallic plates (4).
2. a kind of device for preparing graphene according to claim 1, it is characterised in that the expanded graphite cake (2) is used Suspension bracket is placed in above the first reaction vessel (1).
A kind of 3. device for preparing graphene according to claim 1, it is characterised in that the conductive metal sheet (4) with Reaction vessel uses glue sticking between (1).
4. a kind of device for preparing graphene according to claim 1, it is characterised in that the platinum filament fixed plate (9) is used Suspension bracket is placed in above the second reaction vessel (8).
5. a kind of device for preparing graphene according to claim 1, it is characterised in that weak acid electrolyte (5) is dilute grass The weak acid such as acid or dilute sulfuric acid.
6. a kind of device for preparing graphene according to claim 1, it is characterised in that the first reaction vessel (1) and The material of two reaction vessels (8) is non-conductive.
7. a kind of device for preparing graphene according to claim 1, it is characterised in that conductive metal mesh (3) and conduction The material of metallic plate (4) is copper, iron or aluminium.
CN201720332225.6U 2017-03-25 2017-03-25 A kind of device for preparing graphene Withdrawn - After Issue CN206666136U (en)

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Application Number Priority Date Filing Date Title
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106946242A (en) * 2017-03-25 2017-07-14 哈尔滨摆渡新材料有限公司 A kind of method and device for preparing graphene
CN111514834A (en) * 2020-04-26 2020-08-11 山东沃烯新材料科技有限公司 Ultrasonic wave graphite alkene preparation facility

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106946242A (en) * 2017-03-25 2017-07-14 哈尔滨摆渡新材料有限公司 A kind of method and device for preparing graphene
CN106946242B (en) * 2017-03-25 2019-10-18 哈尔滨摆渡新材料有限公司 A kind of method and device preparing graphene
CN111514834A (en) * 2020-04-26 2020-08-11 山东沃烯新材料科技有限公司 Ultrasonic wave graphite alkene preparation facility

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